CN106553117A - A kind of method that mechanical lapping prepares 20 crystal of spherical super fine ε CL - Google Patents
A kind of method that mechanical lapping prepares 20 crystal of spherical super fine ε CL Download PDFInfo
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- CN106553117A CN106553117A CN201610903649.3A CN201610903649A CN106553117A CN 106553117 A CN106553117 A CN 106553117A CN 201610903649 A CN201610903649 A CN 201610903649A CN 106553117 A CN106553117 A CN 106553117A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B31/00—Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B31/00—Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor
- B24B31/12—Accessories; Protective equipment or safety devices; Installations for exhaustion of dust or for sound absorption specially adapted for machines covered by group B24B31/00
- B24B31/14—Abrading-bodies specially designed for tumbling apparatus, e.g. abrading-balls
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- Mechanical Engineering (AREA)
- Crushing And Grinding (AREA)
Abstract
The invention discloses a kind of method that mechanical lapping prepares 20 crystal of spherical super fine ε CL, the method is comprised the following steps：1) 20 raw materials of ε CL are mixed homogeneously with dispersion liquid, obtains 20 slurries of ε CL；2) 20 slurries of ε CL are input to the grinding intracavity filled with mill ball to be ground；3) 20 slurries of ε CL after grinding are carried out into sucking filtration, drying, obtains 20 crystal of spherical super fine ε CL；The dispersion liquid includes solvent orange 2 A and optional solvent B, and the solvent orange 2 A is selected from least one in ethanol, chloroform, carbon tetrachloride, normal hexane, normal heptane, hexamethylene, 20 recrystallization mother liquor of petroleum ether and ε CL, and the solvent B is water.The method of the present invention can realize the round and smooth of ε CL 20 and refinement simultaneously, also, the purity of 20 crystal of ε CL of the method preparation is high, and the round and smooth degree of crystal is high, even particle size distribution.
Description
Technical field
The present invention relates to contain energy crystal material field, in particular it relates to a kind of mechanical lapping prepares spherical super fine ε-CL-20
The method of crystal.
Background technology
CL-20 (Hexanitrohexaazaisowurtzitane) is the third generation energetic material after RDX, HMX, its quick-fried heat (reason
By value 6.23MJ/kg, density 2.04g/cm3) than HMX (theoretical value 6.19MJ/kg, density 1.91g/cm3) high, the quick-fried heat of volume is carried
It is high by 7.5%.As its density is high, chemistry is good with thermostability, can be with most of composite explosives and propellant additive
It is compatible.Therefore, it is to improve a kind of effective way of composite explosives and the performance of propellant as high energy component with CL-20.For containing
Can material, the factor such as the crystal formation of crystal, crystal morphology, particle size distribution, crystal defect had a major impact to its sensitivity.CL-20 is former
Material sensitivity is high, and crystal form is multi-angular, rough surface, and particle size distribution is uneven, it is impossible to be directly used in composite explosives, propellant and propellant powder
Deng.Spherical super fine ε-CL-20, with lower, the safer characteristic of shock sensitivity and impact sensitivity.Additionally, spherical super fine ε-
CL-20 also has preferable mechanical property.The preparation of spherical super fine ε-CL-20 is to widening the range of application of CL-20, improving weapon
The performance of system is significant.
At present, the method for preparing ultra-fine ε-CL-20 mainly has rapid precipitation method, supercritical fluid recrystallization method, high rapid fire
Stream comminuting method etc., but respectively have its pluses and minuses.
Rapid precipitation method is to make saturated solution with organic solvent dissolving ε-CL-20, then dilute with non-solvent inert fluid
Dispersion is released, explosive is made and is recrystallized with granule crystal state.Ultra-fine ε-the CL-20 for preparing, granularity are typically in micron or Asia
Micron order.Which has the disadvantage high cost, yields poorly；The more difficult control of crystal morphology；Organic solvent requirement is big and is not easily recycled.
Although supercritical fluid technology can prepare ultra-fine explosive crystal, however, this method is present, yield is little, high cost
The characteristics of, it is unfavorable for industrialization and practical application.
High-speed jet comminuting method is the strong punching produced when extremely narrow pipeline high speed flows collision in opposite directions using percussion flow
Hit, extrude, the effect of shearing force, strong turbulence and strong high-pressure sound waves are acted on so that additional load mechanical function is enough more fully hereinafter converted into
Granule is crushed and scattered strength, reaches the purpose of super-refinement.Which has the disadvantage form mist by mutually shock due to solvent
Change drop, this is accomplished by doing liquid very big work(, flow at high speed needs very big pressure to liquid in the duct, and this is close to device
The condition such as envelope property and resistance to pressure requires very high.
In a word, said method exist in various degree complex process, high cost, yield poorly, efficiency is low, the bad control of granularity
System, the shortcomings of crystal morphology is bad, these limit the large-scale production and application of ultra-fine ε-CL-20.
The content of the invention
It is an object of the invention to solve the problems referred to above of prior art presence, ball is prepared so as to provide a kind of mechanical lapping
The method of the ultra-fine ε-CL-20 of shape.
The invention provides a kind of method that mechanical lapping prepares spherical super fine ε-CL-20 crystal, the method includes following
Step：
1) ε-CL-20 raw materials are mixed with dispersion liquid, obtains ε-CL-20 slurries；
2) ε-CL-20 slurries are input to the grinding intracavity filled with mill ball to be ground；
3) ε-CL-20 slurries after grinding are carried out into sucking filtration, drying, obtains the spherical super fine ε-CL-20 crystal；
Wherein, the dispersion liquid includes solvent orange 2 A and optional solvent B, and the solvent orange 2 A is selected from ethanol, chloroform, tetrachloro
Change at least one in carbon, normal hexane, normal heptane, hexamethylene, petroleum ether and ε-CL-20 recrystallization mother liquors, the solvent B is steaming
Distilled water.
The method of the present invention can be by adjusting slurry concentration, stir speed (S.S.), milling time, mill ball material, mill ball
Controlling the pattern and granularity of crystal, the method can realize the round and smooth of ε-CL-20 and refinement to size etc. simultaneously.Also, the party
The purity of ε-CL-20 crystal prepared by method is high, and the round and smooth degree of crystal is high, even particle size distribution.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Exemplary embodiment of the invention is described in more detail by combining accompanying drawing, the present invention it is above-mentioned and its
Its purpose, feature and advantage will be apparent from.
Grain size analysis diagrams of the Fig. 1 for raw material ε-CL-20.
Stereoscan photograph of the Fig. 2 for raw material ε-CL-20.
Fig. 3 is the grain size analysis diagram of spherical super fine ε-CL-20 crystal prepared by embodiment 1.
Fig. 4 is the stereoscan photograph of spherical super fine ε-CL-20 crystal prepared by embodiment 1.
Fig. 5 is the grain size analysis diagram of spherical super fine ε-CL-20 crystal prepared by embodiment 8.
Fig. 6 is the stereoscan photograph of spherical super fine ε-CL-20 crystal prepared by embodiment 8.
Fig. 7 is the stereoscan photograph of spherical super fine ε-CL-20 crystal prepared by embodiment 9.
Specific embodiment
The preferred embodiment of the present invention is more fully described below with reference to accompanying drawings.Although the present invention is shown in accompanying drawing
Preferred implementation, however, it is to be appreciated that may be realized in various forms the present invention and the embodiment party that should not be illustrated here
Formula is limited.Conversely, these embodiments are provided so that the present invention is more thorough and complete, and can be by the present invention's
Scope intactly conveys to those skilled in the art.
The invention provides a kind of method that mechanical lapping prepares spherical super fine ε-CL-20 crystal, the method includes following
Step：
1) ε-CL-20 raw materials are mixed with dispersion liquid, obtains ε-CL-20 slurries；
2) ε-CL-20 slurries are input to the grinding intracavity filled with mill ball to be ground；
3) ε-CL-20 slurries after grinding are carried out into sucking filtration, drying, obtains the spherical super fine ε-CL-20 crystal；
Wherein, the dispersion liquid includes solvent orange 2 A and optional solvent B, and the solvent orange 2 A is selected from ethanol, chloroform, tetrachloro
Change at least one in carbon, normal hexane, normal heptane, hexamethylene, petroleum ether and ε-CL-20 recrystallization mother liquors, the solvent B is steaming
Distilled water.
The method according to the invention, can produce a large amount of foams when individually grinding as dispersion liquid using distilled water, be wrapped in
Blasting explosive granules prevent which from being ground, and affect grinding efficiency, product cut size and distribution, distilled water is mixed with the solvent orange 2 A
When using, or replacing water with the solvent orange 2 A, not only can effectively solving this problem, it is also possible that grinding crystal has preferably
Round and smooth degree and particle size distribution.
In the present invention, the ε-CL-20 recrystallization mother liquors can be the mother solution that solvent-anti-solvent method is recrystallized to give, should
Mother solution can include at least one in ethyl acetate and chloroform, normal heptane, normal octane.
According to one preferred embodiment, the dispersion liquid is selected from ethanol and distilled water, wherein, ethanol and distilled water
Volume ratio is 1 ︰ 0.5～3.
According to another preferred embodiment, the dispersion liquid is ε-CL-20 recrystallization mother liquors, can not only so be improved
The purity of spherical super fine ε-CL-2, moreover it is possible to reduce particle size span.
In the present invention, the concentration of the ε-CL-20 slurries is normally controlled in 10～60 weight %.ε-CL-20 slurries
Concentration is present on product ε-CL-20 size and distribution to be affected：When slurry concentration is too low, it is ground between mill ball medium
Solid particle is few, and the probability that mill ball is contacted with material is low, and its crushing effect is poor；When slurry concentration is too high, slurry viscosity increases
Greatly, material is difficult dispersion.Under preferable case, the concentration of the ε-CL-20 slurries is 28～45 weight %.
In the present invention, the material of the mill ball is may be selected from Achatess, corundum, alumina porcelain, zirconium oxide and politef
At least one.
Normally, the diameter of the mill ball can be 1～12mm, preferably 2～8mm.
In one embodiment, the grinding chamber can include the mill ball of multiple diameter (such as two kinds).
The granularity of ε-CL-20 crystal of the filling rate of the mill ball to preparing also has a great impact：Filling rate is less
When, interstice coverage is easily formed between mill ball, is caused slurry easily " short circuit " to be escaped from, thus crushing effect is poor；When filling rate is higher, slurry
Expect the flow resistance increase in mill chamber, stirring is difficult.In view of preceding factors, and from the angle of reduces cost, the present invention
In, the filling rate of the mill ball is 30～80%, preferably 55～70%.
According to the present invention, the time of the grinding can match somebody with somebody according to the material of mill ball, size, level with the speed of agitator of grinding
Ratio, and the concentration of serosity selected.Normally, the time of the grinding is 30～150min.The stirring of the grinding
Rotating speed can be 10～120r/min.The speed of agitator of the grinding is too high, can cause dangerous increase；Rotating speed is too low, needs
Milling time it is oversize, efficiency step-down.
Under preferable case, the grinding stirring of the present invention so can obtain round and smooth degree higher by the way of first quick and back slow
Crystal and energy saving.Specifically, the grinding is carried out in two stages：
The condition of first stage includes：Speed of agitator is 40～120r/min, and mixing time is 30～90min；
The condition of second stage includes：Speed of agitator is 10～40r/min, and mixing time is 20～60min.
The method of the present invention can be carried out on mechanical lapping equipment commonly used in the art, and the device includes blender
And grinding chamber.
In a particular embodiment, included using the operating process of the inventive method of mechanical lapping equipment：
A) mill ball after match somebody with somebody the certain magnitude for weighing is added in grinding chamber；
B) load weighted raw material ε-CL-20 and dispersion liquid are added in the blender of device, are sufficiently mixed, form uniform
ε-CL-20 slurries；
C) ε-CL-20 slurries are input in grinding chamber and are stirred grinding；
D) discharge valve is opened, releases the ε-CL-20 slurries in grinding chamber, vacuum is carried out to ε-CL-20 slurries then and is taken out
Filter, dries in placing into water-bath baking oven, obtains the spherical super fine ε-CL-20 crystal of drying.
Additionally, the method for the present invention can pass through computer equipment remote control operation all processes and whole video monitor,
To realize automated production.
The method of the present invention can realize the round and smooth of ε-CL-20 raw materials and refinement simultaneously, and operational approach is simple, the ε for obtaining-
CL-20 crystal is micron order (1～15 μm) or submicron order (100nm～1 μm), and plane of crystal is round and smooth, and sphericity is higher.
Specifically, methods described makes ε crystal formation content >=95% in obtained spherical super fine ε-CL-20 crystal, crystal
Median is 0.1～15 μm, particle size span≤0.70, crystalline density >=2.035g/cm3, the short major axis ratio of crystal >=0.8.
Additionally, prepare spherical super fine ε-CL-20 crystal with the inventive method, its yield typically 0.8～1.5 kilogram/
Batch, is generally 30min～150min per the batch used time, the yield and efficiency far above conventional solvent-nonsolvent method and its
Its method.The method of the present invention is capable of achieving remotely control and regulation, it is to avoid in preparation process risk factor to operator with
The security threat for coming.
The present invention is described in detail below by embodiment, but the present invention should not be limited by the examples.
In embodiment and comparative example, raw materials used source is as follows：
ε-CL-20 raw material (crystalline densities 2.0364g/cm3, 95.3%), Liaoning Qingyang special type chemical industry has ε-crystal form purity
Limit company is (as shown in figure 1, d50=125 μm)；
Hexamethylene, Beijing Chemical Plant
Heptane, Beijing Chemical Plant
Normal hexane, Beijing Chemical Plant
Chloroform, Beijing Chemical Plant
Carbon tetrachloride, Beijing Chemical Plant
Ethanol, Tong Guang Fine Chemical Co., Ltd of Beijing
Distilled water, laboratory self-control
(mother solution after laboratory solvent-anti-solvent method recrystallization ε-CL-20, solvent is ε-CL-20 recrystallization saturated solutions
Ethyl acetate, anti-solvent are chloroform).
The particle size distribution of product is characterized with Particle Size Analyzer；Particle size span (S) is calculated according to below equation：
S=(D90-D10)÷(2D50),
Wherein, D10It is by the little granularity accumulated to large volume fraction to 10%.
Crystal form purity is measured using X-ray diffraction method.
Embodiment 1
A) a diameter of 5mm zirconium oxide abrasives balls of 6kg are weighed and a diameter of 3mm zirconium oxide abrasives balls of 3kg is added to grinding chamber
In, filling rate is 60%.
B) 1000g raw material ε-CL-20 are weighed, and 1.5L distilled water and 0.6L ethanol solution are measured in blender, are fully stirred
ε-CL-20 the slurries for making three that mix homogeneously is sufficiently mixed in blender are mixed, ε-CL-20 slurry concentrations are 33.7wt%.
C) above-mentioned ε-CL-20 slurries are input in grinding chamber carries out two benches grinding：First stage agitator speed is
48r/min, milling time are 60min；Second stage agitator speed is 16r/min, and milling time is 30min.
D) grinding chamber discharging opening valve is opened, ε-CL-20 slurries in grinding chamber is put into into suction funnel, recirculated water is then used
Formula vacuum pump sucking filtration is filtered dry, and places into, obtains dry spherical super fine ε-CL-20 products.
Whole preparation process is carried out automatically by remote computer control, whole in real time by Explosionproof camera in control room
The working order of monitoring milling apparatus.
Fig. 3 is the grain size analysis diagram of the ε-CL-20 products；The stereoscan photograph of product as shown in figure 4, as illustrated,
Than more uniform, surface is round and smooth, without obvious corner angle for the granular size of product ε-CL-20.The specific performance of product ε-CL-20 crystal is such as
Shown in table 1.
Embodiment 2～7
Spherical super fine ε-CL-20 crystal is prepared according to the method for embodiment 1, except that, dispersion liquid is replaced with
Different solvents, slurry concentration are 33.7 weight %, so as to spherical super fine ε-CL-20 products are obtained, the species and product of solvent
Performance is as shown in table 1.
Embodiment 8
A) weigh a diameter of 3mm Achatess mill balls of 6.5kg to be added in grinding chamber, filling rate is 65%.
B) 1000g raw material ε-CL-20 are weighed, 2L normal heptane is measured in blender, be sufficiently stirred for making both in blender
ε-CL-20 the slurries of mix homogeneously are sufficiently mixed into inside.ε-CL-20 slurry concentrations are 35%wt.
C) above-mentioned ε-CL-20 slurries are input in grinding chamber and are ground：First stage agitator speed is 64r/
Min, milling time are 70min；Second stage agitator speed is 24r/min, and milling time is 30min.
D) grinding chamber discharging opening valve is opened, ε-CL-20 slurries in grinding chamber is put into into suction funnel, recirculated water is then used
Formula vacuum pump sucking filtration is filtered dry, and places into, obtains dry spherical super fine ε-CL-20 products.
Whole preparation process is carried out automatically by remote computer control, whole in real time by Explosionproof camera in control room
The working order of monitoring milling apparatus.
Fig. 5 is the grain size analysis diagram of the ε-CL-20 products；The stereoscan photograph of product as shown in fig. 6, as illustrated,
Than more uniform, surface is round and smooth, without obvious corner angle, pattern approximate spheres for the granular size of product ε-CL-20.Product ε-CL-20 are brilliant
The specific performance of body is as shown in table 1.
Embodiment 9
(1) weigh a diameter of 3mm zirconium oxide abrasives balls of 10.5kg to be added in grinding chamber, filling rate is 65%.
(2) 1000g raw material ε-CL-20 are weighed, and 1.5L distilled water and 0.6L ethanol solution are measured in blender, are fully stirred
Mix the ε-CL-20 slurries for making both that mix homogeneously is sufficiently mixed in blender.ε-CL-20 slurry concentrations are 33.7%wt.
(3) above-mentioned ε-CL-20 slurries are input in grinding chamber carries out two benches grinding：First stage agitator speed is
64r/min, milling time are 90min；Second stage agitator speed is 36r/min, and milling time is 40min.
(4) grinding chamber discharging opening valve is opened, ε-CL-20 slurries in grinding chamber is put into into suction funnel, then with circulation
Ability of swimming vacuum pump sucking filtration is filtered dry, and places into, obtains dry spherical super fine ε-CL-20.
Whole preparation process is carried out automatically by remote computer control, whole in real time by Explosionproof camera in control room
The working order of monitoring milling apparatus.
The stereoscan photograph of the product as shown in fig. 7, as illustrated, the granular size of product ε-CL-20 is than more uniform,
Surface is round and smooth, without obvious corner angle, pattern approximate spheres.The specific performance of product ε-CL-20 crystal is as shown in table 1.
Embodiment 10
Spherical super fine ε-CL-20 are prepared according to the method for embodiment 1, except that, in step (3), agitator turns
Speed is 64r/min, and the time of grinding is 90min, and so as to spherical super fine ε-CL-20 are obtained, the performance of the product is as shown in table 1.
Comparative example 1
Spherical super fine ε-CL-20 crystal is prepared according to the method for embodiment 1, except that, the dispersion liquid for adopting for
Etc. the water of quality, so as to spherical super fine ε-CL-20 are obtained, the performance of the product is as shown in table 1.
Table 1
From table 1, different grain size can be obtained using the method for the present invention and the more uniform ε-CL-20 of particle size distribution are brilliant
Body, and the method ensure that the ε-crystal formation of CL-20 is not changed substantially, crystal form purity is more than 95%.It is prepared by the present invention
Spherical super fine ε-CL-20 crystal as level adapted granule can be used for composite explosives, propellant, propellant powder etc. mixing medicine in,
To improve energy output.
It is described above various embodiments of the present invention, described above is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.In the case of the scope and spirit without departing from illustrated each embodiment, for this skill
For the those of ordinary skill in art field, many modifications and changes will be apparent from.
Claims (10)
1. a kind of method that mechanical lapping prepares spherical super fine ε-CL-20 crystal, it is characterised in that the method includes following step
Suddenly：
1) ε-CL-20 raw materials are mixed homogeneously with dispersion liquid, obtains ε-CL-20 slurries；
2) ε-CL-20 slurries are input to the grinding intracavity filled with mill ball to be ground；
3) ε-CL-20 slurries after grinding are carried out into sucking filtration, drying, obtains the spherical super fine ε-CL-20 crystal；
Wherein, the dispersion liquid includes solvent orange 2 A and optional solvent B, and the solvent orange 2 A is selected from ethanol, chloroform, four chlorinations
At least one in carbon, normal hexane, normal heptane, hexamethylene, petroleum ether and ε-CL-20 recrystallization mother liquors, the solvent B are distillation
Water.
2. method according to claim 1, wherein, the dispersion liquid is selected from ethanol and distilled water, ethanol and distilled water
Volume ratio is 1 ︰ 0.5～3.
3. method according to claim 1, wherein, the dispersion liquid is ε-CL-20 recrystallization mother liquors.
4. method according to claim 1, wherein, the concentration of the ε-CL-20 slurries is 10～60 weight %, preferably
28～45 weight %.
5. method according to claim 1, wherein, the material of the mill ball is selected from Achatess, corundum, alumina porcelain, oxidation
At least one in zirconium and politef.
6. method according to claim 1, wherein, a diameter of 1～12mm of the mill ball, preferably 2～8mm.
7. method according to claim 1, wherein, the filling rate of the mill ball is 30～80%, preferably 55～
70%.
8. method according to claim 1, wherein, the condition of the grinding includes：Speed of agitator is 10～120r/min,
Mixing time is 30～150min.
9. method according to claim 8, wherein, the grinding is carried out in two stages：
The condition of first stage includes：Speed of agitator is 40～120r/min, and mixing time is 30～90min；
The condition of second stage includes：Speed of agitator is 10～40r/min, and mixing time is 20～60min.
10. method according to claim 1, wherein, methods described makes the ε in obtained spherical super fine ε-CL-20 crystal
Crystal formation content >=95%, the median of crystal is 0.1～15 μm, particle size span≤0.70, crystalline density >=2.035g/cm3,
The short major axis ratio of crystal >=0.8.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107365997A (en) * | 2017-07-13 | 2017-11-21 | 温州万众表面处理技术有限公司 | A kind of polishing agent and preparation method thereof |
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| CN103506194A (en) * | 2012-12-07 | 2014-01-15 | 北京理工大学 | Preparation device and preparation method for ultrafine CL-20 |
| CN105418619A (en) * | 2015-12-29 | 2016-03-23 | 山西北化关铝化工有限公司 | Special hexanitrohexaazaisowurtzitane preparation method |
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| GB1456606A (en) * | 1973-05-15 | 1976-11-24 | Szegvari A | Method and apparatus for grinding particulate solids |
| CN2094394U (en) * | 1991-01-17 | 1992-01-29 | 盘锦化肥厂化工机械分厂 | Vertical metal fine pulverizing ball mill |
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| CN103506194A (en) * | 2012-12-07 | 2014-01-15 | 北京理工大学 | Preparation device and preparation method for ultrafine CL-20 |
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| CN107365997A (en) * | 2017-07-13 | 2017-11-21 | 温州万众表面处理技术有限公司 | A kind of polishing agent and preparation method thereof |
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Application publication date: 20170405 |